MICROSTRUCTURE EXAMINATION OF STEEL

TITLE
Microstructure examination of steel
OBJECTIVE

To observe the constituents and structure of metals and their alloys by means of an optical
microscope.

INTRODUCTION
Microscopic examination with digital imaging Microstructure analysis is conducted by
microscopic examination, a process that studies the structure of materials under magnification.
The properties of a material determine how it will perform under a given application and these
properties are dependent on the materials structure. Industrial processes or treatments such as
casting, welding and heat treating are often applied to metals to prepare them for particular
applications and to improve their characteristics and properties. A microscopic examination may
be conducted to evaluate the effects of a process on material using optical microscopy at low
magnification or scanning electron microscopy (SEM) under high magnification.
There may be residual effects of these processes and treatments, inclusion or contaminants that
can be explained by microstructure analysis and microscopic examination. In many cases, the
investigation centers on the correlation between the resulting microstructure and the material
properties.
Microscopy can give information concerning a materials composition, previous treatment and
properties. Particular features of interest are,

1.
2.
3.
4.
5.

Grain size
Phases present
Chemical homogeneity
Distribution of phases
Elongated structures formed by plastic deformation

For example, exposure of carbon and alloy steels to elevated temperatures during heat
treatment can cause a loss or gain of carbon near the surfaces of the parts if the atmosphere in
the furnace is not properly controlled. Decarburization causes the surface to be soft and weak
with little wear resistance, while unwanted carburization can cause the surface to become too
brittle. Also, if austenitic stainless steel does not see sufficient temperature for enough time or
does not receive a sufficiently rapid quench during heat treating, the carbon in the alloy will
form chromium carbides on the grain boundaries which will make the material brittle and
susceptible to inter granular corrosion. A sensitization test will reveal this problem.

On the other hand, scanning electron microscopy is used to determine abnormalities such as
inclusions, segregation, and surface layers, as well as fracture features. When used in
combination with energy dispersive X-ray spectroscopy (EDS), the microstructure analysis can
identify inclusion type and corrodes on the fracture face.

Microscope (Digital)
A digital microscope is a variation of a traditional optical microscope that uses optics and a
digital camera to output an image to monitor, sometimes by means of software running on
a computer. A digital microscope often has its own in-built LED light source, and differs from
an optical microscope in that there is no provision to observe the sample directly through an
eyepiece. Since the image is focused on the digital circuit the entire system is designed for the
monitor image. The optics for the human eye are omitted.

Digital microscope
THEORY (citation, [Online], Available: http://scitation.aip.org/content/aip/journal)
The theory exhibits all four attributes of normal grain growth: uniformity, scaling, stability, and
lognormality. A prime new feature of the theory is the division of the grains into topological
classes (14 planar, 34 spatial), each with a lognormal distribution of grain sizes. Growth is found
to be controlled by the rate of loss of grains from the lowest topological class. Complete solutions
are found for the grain growth kinetics of each class, as well as the transfer rates between classes.
The latter result is used to explain how the median diameter of those classes in which grains are
shrinking still manages to increase in the manner required to keep their number a constant
2

fraction of the total population. A parabolic growth law is found for the median grain size of the
whole population as well as the median grain size in each topological class. The growth constant
for each class is found to increase approximately as the cube of the planar topological parameter
or the square of the spatial topological parameter. The RhinesCraig structural gradient is shown
to be independent of time and hence a basic constant of normal grain growth. Stability is due to
a maximum in the grain boundary velocity with increasing grain size.

AVERAGE GRAIN INTERCEPT (AGI) METHOD

The average grain intercept (AGI) method is a technique used to quantify the grain - or crystal size for a given material by drawing a set of randomly positioned line segments on the
micrograph, counting the number of times each line segment intersects a grain boundary, and
finding the ratio of intercepts to line length. Thus, the AGI is calculated as: AGI = (number of
intercepts)/(line length). A sample with small crystals will have a high AGI value compared to
a sample with large crystals.

MATERIALS AND APPARATUS

Digital microscope with 50x - 1000x magnification.

Metal specimen
A cleaned cloth
Double disk metal polisher and required diamond paste.

Metal specimen

double disk metal polisher

digital microscope

Diamond paste (with respective colors)

PROCEDURE

First the specimen surface was grind and polished to a smooth and mirror like finish
using disk polisher and diamond paste. Final removal of irregularities is accomplished
by polishing the specimen on a rotating cloth which is covered with extremely fine
abrasive usually diamond paste, until mirror like surface is obtained.
In order to reveal the crystalline structure of the specimen, the polished surface is etched
by a proper etchant. For the Steel, Nitol (2% Nitric Acid) and ethanol is used.
Then it was kept in the digital microscope
The structure of the specimen was captured to a paper.
Then in order to determine grain size a random length was chosen and five lines with the
same length which were parallel to each other was drawn in the scanned paper of
microstructures.
Afterwards the grains covered by each of the drawn lines was counted separately.
Thereafter the number of grains intersected by each line was added and the total was
obtained.
The average grain was calculated after dividing the total of the grains from the number
of lines drawn and by magnification factor.
4

OBSERVATIONS
Grain Size Determination
Length of a line - 10 cm
Number of lines - 5
Number of grains in each of the lines accordingly - 4, 3, 4, 5, 6
Magnification 500X

Some rusted areas were seen in brown color which were randomly oriented.
The surface looked yellowish due to the light which was used to enlighten the area.
Parallel lines were visible due to the scratches uttered while polishing the specimen.
The grain boundaries were not visible as an optical microscope was used.

CALCULATIONS

verage grane size =(

total number of grains

1
)
(no of lines)(length of a line) magnification
22

verage grane size = ( (5)(10) ) 500 = 8.84 104 1

RESULTS

Grain size of the specimen

= 8.84 104 1

DISCUSSION
Process of revealing the crystalline structure of the specimen

Grinding: Is done using rotating discs covered with silicon carbide paper and water. There
are a number of grades of paper, with 180, 240, 400, 1200, grains of silicon carbide per
square inch. 180 grade therefore represents the coarsest particles and this is the grade to begin
the grinding operation. We should always use light pressure applied at the center of the
sample. Continuation of this grinding should be carried out until the blemishes are removed.
Polishing: Is done to get a mirror like surface to clearly observe the structure here it is being
polished by polishers which has rotating discs covered with soft cloth impregnated with a
pre-prepared slurry of hard powdery alumina particles (Al O , the size ranges from 0.5 to
2

0.03 m) and diamond dust.

The specimen should be put in acid in which the acid will attack the grain boundaries taken
into a reaction.
5

Etching: Is done due to Grinding and polishing operations produce a highly deformed, thin
layer on the surface which is removed chemically during etching. Secondly, the etchant
attacks the surface with preference for those sites with the highest energy, leading to surface
relief which allows different crystal orientations, grain boundaries, precipitates, phases and
defects to be distinguished in reflected light digital microscope. This causes light and dark
regions when reflection of light occurs when observing through the microscope.

To calculate the average grain size, the average grain interception method is used. How it is
conducted is initially drawing a set of equal length parallel lines on the micrograph. After that,
counting the number of times the line segment cuts the grain boundary, and thereafter finding
the ratio of intercepts to the line length.

CONCLUSION
In considering the examination of the microstructure, which provides many information
regarding its properties, configuration, and clarifies weather structural parameters are within
certain specifications. The observed results will be useful for the evaluation of the material to be
accepted or rejected. Usually the microstructure examination is performed by an optical or
scanning electron microscope for the magnification process. This examination is conducted in
the industry to identify failure of materials and evaluation specifications. these changes in the
materials properties and processing techniques are very important for the microstructure. So,
metallography has a important place in material science because of interpreting of microsture
and making important changes that effects the physical properties of materials

REFERENCES

Callister Jr W.D., R.D.G. (2010) 'Materials Science and Engineering ' Wiley.
Experiment 3, [Online], Available: http://www.csun.edu/~tarek/EXP3%20Metallography.htm.
Materials Testing, [Online], Available: http://www.labtesting.com/services/materialstesting/metallurgical-testing/microscopic-examination/#sthash.IQ42g0ms.dpuf.
Khel, G.L., Principles of Metallographic Laboratory Practice, McGraw Hill Book Co., (New
York:1949)
William Callister, D., Materials science and engineering, an introduction., (eighth edition)